scholarly journals Determination of Ethyl Carbamate in Commercial Sweetened Sugar Cane Spirit by ESI-MS/MS Using Modified QuEChERS and 18-Crown-6/Trifluoroacetic Acid Spiking Additives

2022 ◽  
Author(s):  
Angélica Tonin ◽  
Camila Poliseli ◽  
Nayane Sinosaki ◽  
Fernanda Martinez ◽  
Oscar Santos ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Aqueous Phase ◽  
Sugar Cane ◽  
Trifluoroacetic Acid ◽  
Limit Of Detection ◽  
Ethyl Carbamate ◽  
Gas Chromatography Mass Spectrometry ◽  
Esi Ms ◽  
Modified Quechers ◽  
Relative Standard

A fast, sensitive, and selective direct injection electrospray tandem mass spectrometry (DI‑ESI‑MS/MS) method that is able to quantify ethyl carbamate in commercial sweetened sugar cane spirit is described. The preparation method uses a modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) with potassium carbonate added to sweetened sugar cane spirit to separate the aqueous phase from the ethanol phase. The aqueous phase contains sucrose that suppresses electrospray ionization. Ethyl carbamate supernatant from the ethanol phase is transferred and enriched with 18-crown-6/trifluoroacetic acid additives. The additives sequester metal cations reducing the ionization of sodium and potassium, favoring the detection of ethyl carbamate as sole protonated cations. The method was successfully applied for the quantification of eleven real samples and certified sugar cane spirit demonstrating its applicability for quality control and regulatory analysis. The method showed reliable analytical parameters compared to conventional gas chromatography mass spectrometry (GC-MS) method commonly used for ethyl carbamate analysis. DI-ESI-MS/MS method requires just a fast step sample clean up and presents consistent values for the limit of detection (LOD 48.0 μg L−1) and limit of quantification (LOQ 160.0 μg L−1). Furthermore, the recoveries obtained were close to 100%, with relative standard deviations below 10% of sample certificates.

scholarly journals Monitoring EDTA and endogenous metabolite biomarkers from serum with mass spectrometry

2005 ◽  
Vol 19 (3) ◽  
pp. 137-146 ◽  
Author(s):  
Rachel Lowe ◽  
Eden P. Go ◽  
Grace C. Tong ◽  
Nicolas H. Voelcker ◽  
Gary Siuzdak
Keyword(s):  
Mass Spectrometry ◽  
Ethylenediaminetetraacetic Acid ◽  
Limit Of Detection ◽  
Free Acid ◽  
Direct Analysis ◽  
Gas Chromatography Mass Spectrometry ◽  
Esi Ms ◽  
C Isotopes ◽  
Endogenous Metabolites

We describe a quantitative method for the determination of ethylenediaminetetraacetic acid (EDTA) in human serum by gas chromatography mass spectrometry (GC-MS), liquid chromatography electrospray ionisation tandem mass spectrometry (LC-ESI-MS/MS), and desorption ionisation on silicon mass spectrometry (DIOS-MS). In the initial stages of the analysis, endogenous metabolites (1-palmitoyl-sn-glycero-3-phosphocholine and 1-stearoyl-sn-glycero-3-phosphocholine) were readily observed in LC-ESI-MS and DIOS-MS however, direct analysis of the EDTA free acid had limited sensitivity. In order to improve EDTA detection we employed a straightforward esterification derivatization. The most successful derivatization procedure converted EDTA to its methyl ester and, since13C isotopes of these reagents are readily available, internal standards could be easily generated for quantitative analysis. This approach provided a limit of detection of 0.5 and 0.1 μM for GC-MS and LC-ESI-MS, and offers a viable method for the EDTA detection.

scholarly journals Single-Laboratory Validation of a Method for the Determination of Furan in Foods by Using Static Headspace Sampling and Gas Chromatography/Mass Spectrometry

2006 ◽  
Vol 89 (5) ◽  
pp. 1417-1424 ◽  
Author(s):  
Patricia J Nyman ◽  
Kim M Morehouse ◽  
Timothy P McNeal ◽  
Gracia A Perfetti ◽  
Gregory W Diachenko
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Apple Juice ◽  
Limit Of Detection ◽  
Peanut Butter ◽  
Gas Chromatography Mass Spectrometry ◽  
Chromatography Mass Spectrometry ◽  
Relative Standard ◽  
Limit Of Quantitation

Abstract A headspace gas chromatography/mass spectrometry method was developed and validated in-house for the determination of furan in foods. The method of standard additions with d4-furan as the internal standard was used to quantitate furan. The limit of detection and limit of quantitation (LOQ) values ranged from 0.2 and 0.6 ng/g, respectively, in apple juice to 0.9 and 2.9 ng/g, respectively, in peanut butter. Recoveries were obtained at 0.5, 1, 2, and 3 times the LOQ. At 1, 2, and 3 times the LOQ, the recoveries ranged from 89.4 to 108%, and the relative standard deviations ranged from 3.3 to 17.3% for all the matrixes. For apple juice, chicken broth, and infant formula, the averaged coefficients of determination from the linear regression analyses were >0.99 with each food fortified at 0.5, 1, 2, and 3 times the LOQ. The coefficients of determination were >0.99 for green beans and 0.96 for peanut butter with the foods fortified at 1, 2, and 3 times the LOQ. Within-laboratory precision was determined by comparing the amounts of furan found in 18 samples by 2 analysts on different days with different instruments. For most of the foods, the difference between the amounts found by each analyst was <18%. The method was used to conduct a survey of >300 foods. The furan levels found ranged from none detected to 174 ng/g.

Rapid Gas Chromatographic Method for Determining Ethyl Carbamate in Alcoholic Beverages with Thermal Energy Analyzer Detection

1988 ◽  
Vol 71 (3) ◽  
pp. 509-511
Author(s):  
Canas Benjamin J ◽  
Donald C HaVery ◽  
Frank L Joe
Keyword(s):  
Mass Spectrometry ◽  
Thermal Energy ◽  
Methylene Chloride ◽  
Limit Of Detection ◽  
Ethyl Carbamate ◽  
Alcoholic Beverages ◽  
Gas Chromatography Mass Spectrometry ◽  
Energy Analyzer ◽  
Elution Method ◽  
Gas Chromatographic Method

Abstract A rapid column elution method has been developed for the determination of ethyl carbamate (EC) in alcoholic beverages. The beverage is mixed with Celite and packed in a column containing deactivated alumina capped with a layer of sodium sulfate. EC is then eluted with methylene chloride. The method, using a gas chromatograph- thermal energy analyzer with a nitrogen converter for detection and quantitation of EC, has been applied to a variety of alcoholic beverages. Recoveries ± standard deviations of EC in wine and whisky fortified at the 20 and 133 µg/kg (ppb) levels averaged 87.3 ± 5.3 and 88.7 ± 3.6%, respectively. The method has a limit of detection of 1.5 ppb. Gas chromatography/mass spectrometry/ mass spectrometry was used to confirm the identity and quantitation of EC in selected beverage extracts.

Ethyl Carbamate Levels in Selected Fermented Foods and Beverages

1989 ◽  
Vol 72 (6) ◽  
pp. 873-876 ◽  
Author(s):  
Benamin J Canas ◽  
Donald C Havery ◽  
Louis R Robinson ◽  
Michael P Sullivan ◽  
frank L Joe ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Limit Of Detection ◽  
Ethyl Carbamate ◽  
Gas Chromatography Mass Spectrometry ◽  
Fermented Foods ◽  
Energy Analyzer ◽  
Gas Chromatograph ◽  
Distilled Spirits ◽  
Mass Spectrometry Mass Spectrometry

Abstract Ethyl carbamate (EC), also known as urethane, is an animal carcinogen and a by-product of fermentation. Because EC has been found in distilled spirits and wines, a variety of fermented foods and beverages were analyzed to assess its occurrence in other products. Previously described methods using a gas chromatograph-thermal energy analyzer with a nitrogen converter were modified for each matrix and gave recoveries of >80%, with a limit of detection in the 1-2 μg/kg(ppb) range. A total of 152 test samples were analyzed; EC levels ranged from none found to 3 ppb in 15 cheeses, 6 teas, 12 yogurts, and 8 ciders; from none found to 13 ppb in 30 breads and 69 malt beverages; and from none found to 84 ppb in 12 soy sauces. Gas chromatography/mass spectrometry/mass spectrometry was used to confirm EC identity and to quantitate EC in selected food extracts

scholarly journals A highly sensitive octopus-like azobenzene fluorescent probe for determination of abamectin B1 in apples

2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Zhenlong Guo ◽  
YiFei Su ◽  
Kexin Li ◽  
MengYi Tang ◽  
Qiang Li ◽  
...  
Keyword(s):  
Fluorescent Probe ◽  
Limit Of Detection ◽  
Quantitative Detection ◽  
Fluorescence Signal ◽  
Ionization Mass ◽  
Limit Of Quantification ◽  
Visible Absorption ◽  
Esi Ms ◽  
Relative Standard ◽  
Ft Ir

AbstractThe development of detecting residual level of abamectin B1 in apples is of great importance to public health. Herein, we synthesized a octopus-like azobenzene fluorescent probe 1,3,5-tris (5′-[(E)-(p-phenoxyazo) diazenyl)] benzene-1,3-dicarboxylic acid) benzene (TPB) for preliminary detection of abamectin B1 in apples. The TPB molecule has been characterized by ultraviolet–visible absorption spectrometry, 1H-nuclear magnetic resonance, fourier-transform infrared (FT-IR), electrospray ionization mass spectroscopy (ESI-MS) and fluorescent spectra. A proper determination condition was optimized, with limit of detection and limit of quantification of 1.3 µg L−1 and 4.4 μg L−1, respectively. The mechanism of this probe to identify abamectin B1 was illustrated in terms of undergoing aromatic nucleophilic substitution, by comparing fluorescence changes, FT-IR and ESI-MS. Furthermore, a facile quantitative detection of the residual abamectin B1 in apples was achieved. Good reproducibility was present based on relative standard deviation of 2.2%. Six carboxyl recognition sites, three azo groups and unique fluorescence signal towards abamectin B1 of this fluorescent probe demonstrated reasonable sensitivity, specificity and selectivity. The results indicate that the octopus-like azobenzene fluorescent probe can be expected to be reliable for evaluating abamectin B1 in agricultural foods.

Simultaneous Determination of Alachlor, Metolachlor, Atrazine, and Simazine in Water and Soil by Isotope Dilution Gas Chromatography/Mass Spectrometry

1989 ◽  
Vol 72 (2) ◽  
pp. 349-354 ◽  
Author(s):  
Lee Q Huang
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Simultaneous Determination ◽  
Isotope Dilution ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
Chromatography Mass Spectrometry

Abstract A multiresidue method was developed for the simultaneous determination of low parts per billion (ppb) concentrations of the herbicides alachlor, metolachlor, atrazine, and simazine in water and soil using isotope dilution gas chromatography/mass spectrometry (GC/MS). Known amounts of 15N,13C-alachlor and 2H5-atrazine were added to each sample as internal standards. The samples were then prepared by a solid phase extraction with no further cleanup. A high resolution GC/low resolution MS system with data acquisition in selected ion monitoring mode was used to quantitate herbicides in the extract. The limit of detection was 0.05 ppb for water and 0.5 ppb for soil. Accuracy greater than 80% and precision better than 4% was demonstrated with spiked samples.

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